CN105017079A - Method for preparing isocyanate in presence of inert solvent - Google Patents
Method for preparing isocyanate in presence of inert solvent Download PDFInfo
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- CN105017079A CN105017079A CN201510350010.2A CN201510350010A CN105017079A CN 105017079 A CN105017079 A CN 105017079A CN 201510350010 A CN201510350010 A CN 201510350010A CN 105017079 A CN105017079 A CN 105017079A
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- inert solvent
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- storage tank
- chiller
- mixture
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000012442 inert solvent Substances 0.000 title claims abstract description 37
- 239000012948 isocyanate Substances 0.000 title claims abstract description 14
- 150000002513 isocyanates Chemical class 0.000 title claims abstract description 13
- 150000001412 amines Chemical class 0.000 claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 239000012071 phase Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 38
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 34
- 238000003860 storage Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 26
- 239000007791 liquid phase Substances 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims description 67
- 238000010791 quenching Methods 0.000 claims description 66
- 150000002148 esters Chemical class 0.000 claims description 54
- 239000008246 gaseous mixture Substances 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 16
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007792 gaseous phase Substances 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 claims description 2
- 229940117389 dichlorobenzene Drugs 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 10
- 239000000443 aerosol Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract 1
- 239000011541 reaction mixture Substances 0.000 description 13
- 239000007787 solid Substances 0.000 description 10
- 239000000376 reactant Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000004985 diamines Chemical class 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- -1 aromatic isocyanate compound Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical group NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of isocyanate preparation and relates to a method for preparing isocyanate in the presence of an inert solvent. The method comprises that an inert solvent and amine are mixed and undergo a reaction with phosgene in a reactor to produce a gas mixture, the gas mixture flows into a chiller and is transformed into a gas-liquid mixture, a chilling agent is sprayed into the chiller, the gas-liquid mixture flows out of an outlet of the chiller and enters into a storage tank, a storage tank gas phase in the storage tank directly enters into a washing tower, and a storage tank liquid phase as an isocyanate product is fed into a rectification refining unit. The method has simple processes, is convenient for operation and has a high energy utilization rate and a low cost. The chiller has a long service life. In chilling, aerosol is not produced. The prepared isocyanate has less impurities and high purity.
Description
Technical field:
The invention belongs to isocyanic ester preparing technical field, relate to a kind of method being prepared isocyanic ester in the presence of an inert solvent by corresponding amine photoreactive gas.
Background technology:
Mainly by corresponding amine and phosgene being carried out prepared by phosgenation for isocyanic ester, phosgenation can be carried out in the liquid phase or in the gas phase, can select to carry out phosgenation in the gas phase in industrial implementation, gas phase phosgenation has a series of advantage compared with liquid phase phosgenation: higher selectivity, the lower phosgene volume of holding and lower cost and energy consumption etc.At present, the existing method very in the gas phase by making corresponding amine and phosgene reaction prepare isocyanic ester, CN1252044C discloses modification method prepared by a kind of isocyanic ester gas phase, wherein a) by general formula R (NH
2)
namine in vapour form, the optional Steam dilution with rare gas element or inert solvent, phosgene is heated to 200 DEG C-600 DEG C, b) amine and phosgene successive reaction is in the reactor made, reactor comprises the reaction chamber not having movement parts, and there is diameter D and center is provided with the nozzle that small aperture is d in reactor, what c) utilize nozzle to make amine parallel with phosgene flows through reactor, and making amine be incorporated in phosgene stream, wherein said amine high cycle speed is in phosgene gas speed and described diameter d and diameter D ratio are 5%-45%; CN1266123C discloses a kind of method preparing isocyanic ester in the gas phase, and the reaction of amine and phosgene is carried out in reaction channel, and the ratio of width to height of the interior dimensions of this reaction channel is at least 2:1; CN1263732C discloses a kind of method that gas phase prepares isocyanic ester, response characteristic in the method in tubular reactor passes through such as homogenizing and determines that the measure relevant to flowing of segregation logistics center realizes, and avoids the formation of the secondary species of the polymerization causing baking deposition and reactor shortening in work-ing life in reactor; CN1064953C discloses the method that gas phase prepares aromatic isocyanate compound, the method comprises to be made at least one contain at least two amine functions figure to contact under excess phosgene exists with phosgene with the compound of at least one aromatic group, two kinds of reactants are sent into gas phase, by the amine function group molar basis of compound, the excessive 0-100% of phosgene.Reaction is carried out in a mixing reactor, and the first homogenizing zone is equivalent to the 20-80% of reactor cumulative volume, and second segment is equivalent to the 80-20% of reactor cumulative volume, and in second segment, logistics is close to piston flow; CN1317262C discloses the method that one prepares (many) isocyanic ester in the gas phase, in the method, vaporous diamines can with rare gas element or the Steam dilution with inert solvent, phosgene is heated to separately about 200-600 DEG C, mix in tubular reactor and react, the nozzle that n >=2 are parallel to tubular reactor axle is set in tubular reactor, by a described n nozzle, the air-flow comprising diamines is passed in described tubular reactor, phosgene is passed in described tubular reactor by remaining freeboard simultaneously; CN101258127B discloses a kind of method preparing isocyanic ester, n stock amine stream and n+1 stock phosgene stream is made to react in the reactor in the method, wherein n be at least 1 positive integer, and all amine photoreactive gas streams are mixed via annular interval introducing reactor, wherein these annular interval arrangements each other should be make their center of gravity be located substantially on straight line, and the center of gravity wherein protruding into the circular clearance of annular clearance space is farthest positioned on the major axis of annular clearance space; CN101848890B discloses a kind of method of producing isocyanic ester, in the method, by corresponding amine and phosgene, optionally react in the gas phase under the existence of at least one inert media, by making the fluid streams of amine photoreactive gas contact and make them react to each other subsequently and prepare isocyanic ester, it comprises the fluid be just arranged on the wall of flow passage by least one before at least one stream contacts with the another kind of stream interference unit that flows and reduces the turbulent flow interface of described at least one stream; CN101796022A discloses a kind of method preparing isocyanic ester, amine, phosgene is wherein made to contact at least one mixing device with the fluid of inert media, then make amine and phosgene react to each other, in mixing device, at least between an amine stream and a phosgene stream, be metered into inert media.
Can know from above-mentioned published method, the temperature of the reaction mixture in gas phase after the phosgenation of amine photoreactive gas is 400-600 DEG C, reaction product isocyanic ester is easy to react and generates solid at this high temperature, not only reducing product yield also can cause the blocking impact of reactor to produce, so reaction mixture must cool by fast cooling after reaching optimum reacting time, prevent the generation of isocyanate reaction, high-temperature gas carries out fast cooling method by spraying into liquid is called Quench (quenching), and the region that Quench occurs is called chiller, CN1496977 discloses the method for quenching of gas reaction mixture in a kind of diamines gas phase phosgenation process, at least two nozzles are used to inject quench liquid when gaseous mixture flows out into round shape quenched region, downstream continuously from barrel type reactor in the method, nozzle is along the equidistant ingress being arranged in quenched region of quenched region periphery, and wherein quencher liquid temp is 100-170 DEG C, CN101595086A discloses a kind of by making amine and phosgene react in the gas phase at least one reaction zone, make reaction mixture inject at least one liquid wherein by least one and produce the method for isocyanic ester to stop the district of described reaction, this reaction mixture is by being full of the continuous quench liquid curtain of quench region cross section completely, CN1015325242B discloses and a kind ofly wherein injects by carrying out reacting at least one reaction zone in the gas phase and reaction mixture being sent at least one at least one liquid to produce isocyanic ester method with the district of termination reaction by corresponding amine photoreactive gas, between reaction zone and the district of wherein reaction terminating, there is the district with expansion or section of constant cross section, the method of isocyanic ester is prepared in the reaction that CN101200437B discloses primary amine photoreactive gas in the gas phase, wherein, by reaction mixture is made described reaction terminating from the cooling extension of reaction chamber pilot flow through there being liquid to inject, in the cooling zone of the two or more series connection in cooling extension, directly cool within a stage, CN102239143B discloses a kind of method preparing isocyanic ester, by optionally in the presence of an inert media, corresponding amine and phosgene is made to react under gas phase and carry out, wherein first amine photoreactive gas mixes and reacts generation isocyanic ester in the reactor, by adding liquid quench medium, the reactant gases comprising isocyanic ester and hydrogenchloride leaving described reactor is cooled in quencher, thus the mixture forming a kind of reactant gases and quench medium is as product stream, quench medium used is a kind of mixture comprising at least one solvent and described isocyanic ester shifted out from preparation process, quench medium removed solid particulate wherein before adding quencher, CN102272095A discloses a kind of method preparing isocyanic ester, wherein optionally in the presence of an inert media, corresponding amine and phosgene are reacted in the gas phase, wherein first amine photoreactive gas mixes and is converted into isocyanic ester in the reactor, the reactant gases comprising isocyanic ester and hydrogenchloride wherein leaving described reactor cools by adding liquid quench medium in quencher, thus form the mixture of a kind of reactant gases and quench medium, the amount of the quench medium added makes the temperature of the mixture of reactant gases and quench medium---described temperature and quencher balance---higher than the dew point of gas contained in described quencher.
The method that can reduce reaction mixture temperature in prior art fast uses spray method to carry out Quench cooling, the temperature of reaction mixing section thing can be reduced at short notice by this method, in spray method disclosed in CN101535242, chill time can reach in 0.2s, but the method subject matter is because between reaction product and Quench agent, the temperature difference is high, aerosol can be formed by spray pattern rapid cooling, the aerosol formed is difficult to process, simultaneously in prior art, chilling process major part is all that liquid phase material after using reaction mixture Quench is as Quench agent, this method has two shortcomings, first is have solid after reaction mixture Quench to produce, directly solid can be made to enter in spray nozzle as Quench agent the material after Quench, cause the blocking of nozzle, due to the key equipment that nozzle is chilling process, spray nozzle clogging can cause Quench agent flux to reduce, the problems such as spray droplet skewness, cause Quench can not reach the object reducing reaction mixture temperature fast, second is that the concentration of isocyanic ester in liquid after reaction mixture Quench can arrive more than 50%, is easy to generate solid and result in blockage to chilling facility after the isocyanic ester of such high density contacts with pyroreaction mixture.For aerosol problem, CN102272095A employs more than the dew-point temperature of temperature contained gas in chiller after Quench, to avoid aerocolloidal generation, but the bad control of the amount adding Quench agent, and liquid formation is inevitably had when step of reaction has fluctuation, too high and the solids problem for isocyanate concentration in Quench agent, the method that CN102239143B uses falls solid by adding a metre filter before Quench agent enters chiller, use partial reaction mixture phlegma simultaneously, entering the solvent added in the agent of chiller forward direction Quench in Quench agent, to reduce the concentration of isocyanic ester in Quench agent, in order to the particle removed in the agent of circulation Quench needs to add a strainer, filter stoppage can cause produces instability, simultaneously in order to the concentration reducing isocyanic ester in Quench agent needs to add a large amount of solvent, increase the energy consumption of last handling process.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence, seeking to design provides a kind of method preparing isocyanic ester in the presence of an inert solvent, solve the aerosol problem produced in chilling process, reduce the concentration of isocyanic ester in Quench agent, avoid the existence of solid particulate in Quench agent, extend the work-ing life of chiller, and without the need to strainer, production process is stable.
To achieve these goals, the present invention chooses conventional isocyanic ester preparation system and device, the specific embodiment preparing isocyanic ester is: inert solvent and amine are mixed to get the mixture of inert solvent and amine according to the ratio that mass ratio is 0.5-5:1, mixture photoreactive gas hybrid reaction in reactor of inert solvent and amine obtains gaseous mixture, the amino mol ratio entered in the phosgene of reactor and the mixture of inert solvent and amine is 1.2-5:1, before entering reactor, the mixture of phosgene and inert solvent and amine is all heated to 250 DEG C-400 DEG C, in reactor, temperature is 300 DEG C-500 DEG C, pressure is 0.3-3barA, gaseous mixture flows into chiller after reactor flows out, Quench agent enters chiller with spray pattern, in chiller, the temperature of gaseous mixture is down to less than 200 DEG C in 0.1s, liquid phase is entered after isocyanic ester cooling in gaseous mixture, the solvent contained in Quench agent is gasificated as gas phase, gaseous mixture becomes gas-liquid mixture, gas-liquid mixture flows out from the outlet of chiller and enters storage tank, storage tank gas phase in storage tank directly enters washing tower, storage tank liquid phase in storage tank sends into external rectified purified unit as isocyanate products, after storage tank gas phase enters washing tower, the isocyanic ester contained in storage tank gas phase and partial solvent are washed down as tower reactor absorption liquid, phosgene, hydrogenchloride and remaining solvent leave as top gaseous phase from washing tower tower top and enter condenser and carry out condensation, the tower top liquid phase that condensation is got off enters the tower top of washing tower as washing composition, condenser gas phase in condenser is sent into external gas recovery processing unit and is recycled, the tower reactor absorption liquid of washing tower enters heat exchanger by pump delivery, tower reactor absorption liquid is heated or is condensed to 5-20 DEG C lower than the bubble point temperature of inert solvent under chiller internal pressure after over-heat-exchanger, tower reactor absorption liquid through over-heat-exchanger enters chiller as Quench agent and recycles, now, in Quench agent, the weight percent content of isocyanic ester is less than 10%.
Inert solvent of the present invention comprises the one in toluene, chlorobenzene, dichlorobenzene and dimethylbenzene; Solvent in Quench agent is identical with inert solvent, and the temperature of Quench agent is 120-180 DEG C.
The present invention compared with prior art, has the following advantages: one is use the absorption liquid of washing tower as Quench agent, ensures do not have solid particulate in Quench agent; Two is directly enter a washing tower after the gas phase left from chiller enters storage tank to wash, and solves the aerocolloidal problem produced in chilling process; Three is because isocyanic ester most of in chiller enters liquid phase, so the massfraction of isocyanic ester is less than 10% in Quench agent, avoids like this producing solid in chiller nozzle and chiller; Four is that patent CN102272095A dilutes in order to the concentration reducing isocyanic ester in Quench agent adds inert solvent before Quench agent enters chiller, inert solvent is added in the logistics of the present invention when reacting at amine, the gas phase that after the reaction of amine photoreactive gas, Quench obtains in chiller is absorbed liquid as Quench agent after washing, obtain the Quench agent of low isocyanate concentration like this, add the concentration that inert solvent can reduce amine in the reaction, avoid amine and isocyanic ester to react production impurity; Its technique is simple, and easy to operate, energy utilization rate is high, and cost is low, chiller long service life, and chilling process does not produce aerosol, and the isocyanate impurities prepared is few, and purity is high.
Accompanying drawing illustrates:
Fig. 1 is the technical process principle schematic that the present invention prepares isocyanic ester, and wherein A is reactor, and B is chiller, and C is storage tank, D is washing tower, and E is condenser, and F is pump, G is heat exchanger, and 1 is phosgene, and 2 is the mixture of inert solvent and amine, 3 is gaseous mixture, and 4 is gas-liquid mixture, and 5 is storage tank gas phase, 6 is storage tank liquid phase, and 7 is top gaseous phase, and 8 is condenser gas phase, 9 is tower top liquid phase, and 10 is tower reactor absorption liquid, and 11 is Quench agent
Embodiment:
Below by embodiment, also the invention will be further described by reference to the accompanying drawings.
The specific embodiment that the present embodiment prepares isocyanic ester is: by the mixture 2 being mixed to get inert solvent and amine according to the mass ratio ratio that is 0.5-5:1 of inert solvent and amine, mixture 2 photoreactive gas 1 hybrid reaction in reactor A of inert solvent and amine obtains gaseous mixture 3, the amino mol ratio entered in the phosgene 1 of reactor A and the mixture 2 of inert solvent and amine is 1.2-5:1, before entering reactor A, the mixture 2 of phosgene 1 and inert solvent and amine is all heated to 250 DEG C-400 DEG C, in reactor A, temperature is 300 DEG C-500 DEG C, pressure is 0.3-3barA, gaseous mixture 3 flows into chiller B after reactor A flows out, Quench agent 11 enters chiller B with spray pattern, in chiller B, gaseous mixture 3 temperature in 0.1s is down to less than 200 DEG C, liquid phase is entered after isocyanic ester cooling in gaseous mixture 3, the solvent contained in Quench agent 11 is gasificated as gas phase, gaseous mixture 3 becomes gas-liquid mixture 4, gas-liquid mixture 4 flows out from the outlet of chiller B and enters storage tank C, storage tank gas phase 5 in storage tank C directly enters washing tower D, storage tank liquid phase 6 in storage tank C sends into external rectified purified unit as isocyanate products, after storage tank gas phase 5 enters washing tower D, the isocyanic ester contained in the gas phase contained in storage tank gas phase 5 and partial solvent are washed down as tower reactor absorption liquid 10, phosgene, hydrogenchloride and partial solvent leave as top gaseous phase 7 from washing tower D tower top and enter condenser E and carry out condensation, the tower top liquid phase 9 that condensation is got off enters the tower top of washing tower D as washing composition, condenser gas phase 8 in condenser E is sent into external gas recovery processing unit and is recycled, the tower reactor absorption liquid 10 of washing tower D delivers into heat exchanger G by pump F, tower reactor absorption liquid 10 is heated or is condensed to 5-20 DEG C lower than the bubble point temperature of inert solvent under chiller B internal pressure after over-heat-exchanger G, tower reactor absorption liquid 10 through over-heat-exchanger G enters chiller B as Quench agent 11 and recycles, now, in Quench agent 11, the weight percent content of isocyanic ester is less than 10%.
Embodiment:
The inert solvent that the present embodiment uses is chlorobenzene, amine is 1, 6-hexanediamine (HDA), the mass ratio of chlorobenzene and HDA is 2.4:1, chlorobenzene and HDA are heated to 300 DEG C, phosgene is heated to 300 DEG C, gaseous mixture and the phosgene of chlorobenzene and HDA pass into reactor A simultaneously, in reactor A, after mixing, reaction generates hexamethylene diisocyanate (HDI) and HCL, reactor A temperature is 400 DEG C, from reactor A gaseous mixture 3 flow 2800kg/h out, in gaseous mixture 3, the massfraction of isocyanic ester is 20%, in gaseous mixture 3, the massfraction of chlorobenzene is 35.1%, in chiller B, the temperature of gaseous mixture 3 drops to 150 DEG C from 400 DEG C, Quench agent 11 temperature used is 120 DEG C, Quench agent 11 flow is 3350kg/h, in Quench agent 11, isocyanate mark is 6%, gas-liquid mixture 4 flows into storage tank C from chiller B, the gas phase flow rate entering washing tower D from storage tank C top is 5300kg/h, the gas phase flow rate left from washing tower D top is 1950kg/h, tower reactor absorption liquid 10 flow that washing tower D tower reactor flows out is 3350kg/h, tower reactor absorption liquid 10 recycles as Quench agent 11, in Quench agent 11, the massfraction of isocyanic ester is 6.1%, in the storage tank liquid phase 6 of storage tank C, the concentration of isocyanic ester is 64.2%, storage tank liquid phase 6 is delivered to downstream units as the thick product of isocyanic ester and is carried out refinement treatment.
Claims (2)
1. prepare the method for isocyanic ester in the presence of an inert solvent for one kind, it is characterized in that the specific embodiment preparing isocyanic ester is: inert solvent and amine are mixed to get the mixture of inert solvent and amine according to the ratio that mass ratio is 0.5-5:1, mixture photoreactive gas hybrid reaction in reactor of inert solvent and amine obtains gaseous mixture, the amino mol ratio entered in the phosgene of reactor and the mixture of inert solvent and amine is 1.2-5:1, before entering reactor, the mixture of phosgene and inert solvent and amine is all heated to 250 DEG C-400 DEG C, in reactor, temperature is 300 DEG C-500 DEG C, pressure is 0.3-3barA, gaseous mixture flows into chiller after reactor flows out, Quench agent enters chiller with spray pattern, in chiller, the temperature of gaseous mixture is down to less than 200 DEG C in 0.1s, liquid phase is entered after isocyanic ester cooling in gaseous mixture, the solvent contained in Quench agent is gasificated as gas phase, gaseous mixture becomes gas-liquid mixture, gas-liquid mixture flows out from the outlet of chiller and enters storage tank, storage tank gas phase in storage tank directly enters washing tower, storage tank liquid phase in storage tank sends into external rectified purified unit as isocyanate products, after storage tank gas phase enters washing tower, the isocyanic ester contained in storage tank gas phase and partial solvent are washed down as tower reactor absorption liquid, phosgene, hydrogenchloride and remaining solvent leave as top gaseous phase from washing tower tower top and enter condenser and carry out condensation, the tower top liquid phase that condensation is got off enters the tower top of washing tower as washing composition, condenser gas phase in condenser is sent into external gas recovery processing unit and is recycled, the tower reactor absorption liquid of washing tower enters heat exchanger by pump delivery, tower reactor absorption liquid is heated or is condensed to 5-20 DEG C lower than the bubble point temperature of inert solvent under chiller internal pressure after over-heat-exchanger, tower reactor absorption liquid through over-heat-exchanger enters chiller as Quench agent and recycles, now, in Quench agent, the weight percent content of isocyanic ester is less than 10%.
2. prepare the method for isocyanic ester according to claim 1 in the presence of an inert solvent, it is characterized in that described inert solvent comprises the one in toluene, chlorobenzene, dichlorobenzene and dimethylbenzene; Solvent in Quench agent is identical with inert solvent, and the temperature of Quench agent is 120-180 DEG C.
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| CN201510350010.2A CN105017079B (en) | 2015-06-24 | 2015-06-24 | A kind of method preparing isocyanates in the presence of an inert solvent |
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| CN201510350010.2A CN105017079B (en) | 2015-06-24 | 2015-06-24 | A kind of method preparing isocyanates in the presence of an inert solvent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108246050A (en) * | 2016-12-29 | 2018-07-06 | 重庆长风生物科技有限公司 | A kind of vapor phase method prepares the cooling device and method of HDI |
| CN114044745A (en) * | 2021-12-06 | 2022-02-15 | 甘肃银光聚银化工有限公司 | Method for synthesizing 1, 5-pentamethylene diisocyanate by gas phase phosgenation method |
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| CN101200437A (en) * | 2006-12-13 | 2008-06-18 | 拜尔材料科学股份公司 | Method for producing isocyanates in the gas phase |
| CN101535242A (en) * | 2006-11-07 | 2009-09-16 | 巴斯夫欧洲公司 | Method for producing isocyanates |
| CN102239143A (en) * | 2008-12-03 | 2011-11-09 | 巴斯夫欧洲公司 | Method for producing isocyanates |
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2015
- 2015-06-24 CN CN201510350010.2A patent/CN105017079B/en not_active Expired - Fee Related
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| WO2008055904A1 (en) * | 2006-11-07 | 2008-05-15 | Basf Se | Method for producing isocyanates |
| CN101535242A (en) * | 2006-11-07 | 2009-09-16 | 巴斯夫欧洲公司 | Method for producing isocyanates |
| CN101200437A (en) * | 2006-12-13 | 2008-06-18 | 拜尔材料科学股份公司 | Method for producing isocyanates in the gas phase |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108246050A (en) * | 2016-12-29 | 2018-07-06 | 重庆长风生物科技有限公司 | A kind of vapor phase method prepares the cooling device and method of HDI |
| CN114044745A (en) * | 2021-12-06 | 2022-02-15 | 甘肃银光聚银化工有限公司 | Method for synthesizing 1, 5-pentamethylene diisocyanate by gas phase phosgenation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105017079B (en) | 2016-11-23 |
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